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Catalyst In Situ Generated Sio <sub> 2 </ Sub> Structure Of The Particles And (peo) <sub> 8 </ Sub> Of Liclo <sub> 4 </ Sub>-sio <sub> 2 </ Sub> Composite Things Membrane Performance

Posted on:2008-05-27Degree:MasterType:Thesis
Country:ChinaCandidate:Q ZhangFull Text:PDF
GTID:2191360215985109Subject:Organic Chemistry
Abstract/Summary:PDF Full Text Request
Firstly, in order to understand the effects of the process of SiO2 particle growth, taking ethyl-orthosilicate (TEOS) as the precursor, SiO2 sol, PEO/SiO2 and (PEO)8LiClO4-SiO2 were prepared by blending in-situ. And the influences of polymer, lithium salt, catalyst in the process of SiO2 particle growth were inspected. The growth of the nanometer particle SiO2 were studied by Ultraviolet-Visible light spectrophotometer, transmission electron microscope (TEM), atom force microscopy(AFM). Secondly, we studied the effects of structure of SiO2 in the properties of (PEO)8LiClO4-SiO2 composites. (PEO)8LiClO4-SiO2 composites were prepared by blending in situ, which ethyl-orthosilicate (TEOS) was catalyzed both by HCl and NH4OH. The crystallinity and ionic conductivity of the CSPE were investigated by different scanning calorimeter(DSC), X-Ray diffracts (XRD) and A.C.impedance spectroscopy. The gas sensitivity and the surface properties of (PEO)8LiClO4-SiO2 composites were studied too.The results of Ultraviolet-Visible light spectrophotometer show that the acid-catalyzed SiO2 sol is stabler than the alkali-catalyzed SiO2 sol. The acid-catalyzed SiO2 sol. The results of TEM show that under the SiO2 sol system, the size of SiO2 particle is approximately 35nm, the shape is not really regular, particles agglomerate partly and size distribute widely. Under PEO/SiO2 system, PEO surround the SiO2 particle formed core-shell structure, the average particle size is about 100nm.Under the (PEO)8LiClO4-SiO2 system, the results of AFM show that SiO2 particles in the acid-catalyzed (PEO)8LiClO4-SiO2 film surface results are not so protuberant as SiO2 particles in the acid-catalyzed (PEO)8LiClO4-SiO2 film surface. The height of SiO2 in acid-catalyzed (PEO)8LiClO4-SiO2 film is 18.8nm; the height of SiO2 in alkali-catalyzed (PEO)8LiClO4-SiO2 film is 80.5nm. The results of TEM show that both alkali-catalyzed SiO2 particles and alkali-catalyzed SiO2 particles with the sizes of 50~100nm were quite well dispersed in the CSPE. The figure of alkali-SiO2 particles was round and the interfaces were conspicuous. The figure of acid-catalyzed SiO2 particles was not regular and the interfaces were unconspicuous. Both the results of AFM and TEM indicate the compatibility of acid- catalyzed SiO2 in CSPE is better than alkalicatalyzed SiO2.DSC and XRD show that the crystallinity of acid-catalyzed (PEO)8LiClO4-SiO2 and alkali-catalyzed (PEO)8LiClO4-SiO2 are 8.6% and 10.2 % respectively. The crystallinity is observed to decrease greatly by addition of modified SiO2. A. C. impedance spectra of CSPE shows that the conductivity is increased obviously by addition of SiO2 at room temperature. When SiO2 concentration is at about 10wt%, the conductivity of alkali-catalyzed CSPE and acid-catalyzed CSPE attains the maximum value. The conductivity of alkali-catalyzed CSPE and acid-catalyzed CSPE are 1.1×10-5 S·cm-1 and 2.2×10-5 S·cm-1 respectively at 30℃. The gas sensitivity testing show that the responsive resistance of acid-catalyzed (PEO)8LiClO4-SiO2 is 717.1KΩin air and 508.1KΩin ethanol; the responsive resistance of alkali-catalyzed (PEO)8LiClO4-SiO2 is 2792. 1KΩin air and 796.6KΩin ethanol. The smaller the bulk resistance is, the bigger the conductivity is. The conductivity of acid-catalyzed (PEO)8LiClO4-SiO2 is bigger than alkali-catalyzed (PEO)8LiClO4-SiO2 which is consistent with the results of A. C. impedance spectra. The results of contact angle testing show that the ionic conductivity is related to the surface flee energy, the smaller the surface free energy is, the bigger the ionic conductivity is; the bigger the surface free energy is, the smaller the ionic conductivity is.
Keywords/Search Tags:PEO, SiO2, Composite polymer electrolyte, Ionic conductivity
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